EP0239280A2 - Revêtement de protection pour films de protection solaire - Google Patents

Revêtement de protection pour films de protection solaire Download PDF

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Publication number
EP0239280A2
EP0239280A2 EP87302029A EP87302029A EP0239280A2 EP 0239280 A2 EP0239280 A2 EP 0239280A2 EP 87302029 A EP87302029 A EP 87302029A EP 87302029 A EP87302029 A EP 87302029A EP 0239280 A2 EP0239280 A2 EP 0239280A2
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EP
European Patent Office
Prior art keywords
film
tin oxide
nitride
titanium nitride
glass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP87302029A
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German (de)
English (en)
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EP0239280A3 (en
EP0239280B1 (fr
Inventor
Roy Gerald Gordon
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Individual
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Publication of EP0239280A3 publication Critical patent/EP0239280A3/en
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
    • G02B1/105—
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/14—Protective coatings, e.g. hard coatings

Definitions

  • This invention relates to the improvement of titanium nitride films, particularly those used in shielding windows from excessive heat gain during warm weather.
  • a principal object of the invention is to provide an oxidation-resistant protective layer over a thin, transparent, titanium-nitride-bearing film.
  • Another object of the invention is to provide oxidation protection of TiN film during high-­temperature processing of glass sheets upon which the film has been deposited.
  • Another object of the invention is to provide a titanium nitride-based solar film which has excellent abrasion resistance.
  • Still further objects of the invention are to provide solar-control products having superior light-­attenuating characteristics, particularly reduced visible reflectivity and reduced color.
  • Another object of the invention is to provide an improved and more efficient process for using TiN as a solar shield on architectural windows, to reduce the solar heat gain during hot weather.
  • a protective transparent film advantageously tin oxide.
  • a protective transparent film advantageously tin oxide.
  • sili­con oxide, and aluminum oxide also have good protec­tive properties.
  • tin oxide, particularly fluorine-doped tin oxide is believed to have the most favorable combination of mechanical, optical, and infrared emissivity properties to complement solar-­shield applications.
  • titanium nitride can be replaced as the pri­mary solar absorption film, in whole or in part, with solar screening nitrides such as nitrides VN, NbN, TaN, CrN and Cr3N4 as described in U.S. Patent 3,885,855.
  • solar screening nitrides such as nitrides VN, NbN, TaN, CrN and Cr3N4 as described in U.S. Patent 3,885,855.
  • Titanium nitride coating is the most advantageous choice for most applications because of the relative ease with which gaseous precursors to the coating can be formed and handled on processing equipment.
  • the thinner tin oxide films i.e, those of about 500 angstroms thick, are preferable for use on high-­ligh-transmission glass sheets, e.g., those over a 300 angstrom thick TiN film.
  • high-­ligh-transmission glass sheets e.g., those over a 300 angstrom thick TiN film.
  • An example would be pri­mary vision areas of automotive glass which would have a visible light transmission of about 70%. In such an instance, total solar transmission would be about 50%.
  • a tita­nium nitride thickness of about 600 to 1000 angstroms again in combination with a 500 angstrom overcoat film of tin oxide, would provide a highly-suitable com­bination for obtaining a 15% visible transmission and 8% transmission of total solar transmission.
  • transparent glass sheets comprising thereon titanium-­nitride as the principal solar screening layer for reducing transmission of near infrared and, thereover, a layer of tin oxide of about 300 to 800 angstroms thick.
  • the tin oxide layers serves to protect the titanium nitride from oxidation during high-­temperature processing procedures, increases the abrasion-resistance, and, at 500 angstroms or roughly the midpoint of the 300 to 800 angstrom range, is use­ful in reducing the color and reflectivity properties of some titanium nitride films.
  • some of the tin oxide that is not require for physical pro­tection of the TiN or visual effect, can be positioned between the nitride and the glass substrate.
  • the performance of these compound solar-control coating is only slightly dependent on the glass substrate on which they are placed. However, more exact values of optimum thickness can be determined for an individual application of the invention after one selects a particular substrate and the desired parameters for emissivity and solar transmission values.
  • the titanium-nitride based, or chromium-­nitride based, coating is sandwiched between two pro­tective oxide coatings, e.g., two tin-oxide coatings.
  • the titanium nitride film serves the principal function of reducing near-infrared (wavelengths of from about 0.7 to 2 microns) transmission.
  • the outer layer of tin oxide serves to increase the abrasion resistance and serves as an oxidation-protective layer during manufacture, after the coating operation itself, in subsequent, high-­temperature fabrication steps such as annealing, tem­pering or bending processes.
  • the inner layer of tin oxide that layer posi­tioned between the glass substrate and the titanium nitride, promotes a desirably uniform nucleation of the titanium nitride during the deposition of TiN and serves to insulate the TiN from any undesirable chemi­cal interaction with the glass substrate.
  • Both tin oxide layers serve to increase the ratio of transmission of visible light to the transmission of near infrared light because of their high refrac­tive index.
  • the tin oxide films are also particularly effective in reducing emissivity (reflecting far-­infrared) when they have been fluorine-doped according to manufacturing procedures known in the art.
  • the tin oxide films total about 1000 angstroms in thickness.
  • each tin oxide film may be about 500 angstroms thick.
  • TiN films those with otherwise highly desirable shading characteristics for some architec­tural use, have, taken alone on a glass substrate, reflection characteristics which are aesthetically undesirable. Similar problems are encountered with chromium nitride films. Thus, TiN films of about 1750 angstroms in thickness have an almost mirror-like bluish reflection color from the coated side. This is particularly true when the coating is formed according to the process described by Gordon in U.S. Patent 4,535,000, i.e., by reacting ammonia and titanium chloride. When a tin oxide film of about 575 angstroms is placed on top of the TiN, the reflected color becomes virtually undetectable to most obser­vers. Indeed, the highly reflective nature of the transparent sheet also drops markedly, roughly approximating the reflectance of untreated architec­tural glass. Such reflection-diminished film will have a visible transmission of about 5-6% with a total solar transmission that is even lower.
  • transparent glass products prepared according to the invention can be annealed at typical glass-plate annealing tem­peratures of about 1100°F for an hour without any significant, or even detectable, oxidation of the solar-control film.
  • tempering at tem­peratures of about 1150°F for five minutes results in no deterioration of the product. Similar testing was carried out by measuring the contact resistance bet­ween the tin oxide film, through the TiN layer, to a silicon substrate. Any oxidation of the TiN would have resulted in a large increase in the electrical contact resistance measured during the test.
  • Another important process aspect of the invention is the conservation of titanium nitride, or like nitrides, which would otherwise be lost to oxidation during the process of coating hot glass with TiN according to such high-temperature procedures as are illustrated by the process disclosed in U.S. Patent 4,535,000.
  • the titanium nitride film would take about 20 seconds to move 10 feet from the exit of the tin float bath to the tin oxide over coating, then about 100 to 150 angstroms of the top surface of titanium oxide could be oxidized to tita nium oxide.
  • Such a loss of TiN can often be tolerated or compensated for. But, it introduces a wholly unnecessary variable into the pro­cess.
  • the tin oxide is of particular value in avoiding the above-described loss of nitride during the coating operation. Such conversion of nitride to oxide also introduces another variable into the product and may result in color variations in product as it is sub­jected to post-coating annealing and tempering.
  • the tin oxide offers particular value in protecting the newly-formed TiN from oxidation during annealing and tempering operations at temperatures exceeding 800°F and, typically between 1000 and 1200°F.
  • the overcoating of the nitride with tin oxide is advantageously carried out in the non-­oxidizing atmosphere of the tin bath structure in which the glass sheet to be coated is formed. This procedure allows the required amount of nitride to be used more efficiently as a solar shield and to be deposited more rapidly because no significant allowance need be made for oxidation.
  • the titanium nitride deposited on the glass of Figures 1 and 2 is deposited according to the process described in U.S. Patent 4,535,000.
  • the tin oxide is a fluorine-doped oxide and deposited according to the process described in U.S. Patent 4,146,657.
  • the structure according to Figure 1 was modified by replacing the tin oxide with silicon oxide, in one instance, and aluminum oxide in another instance. Both of these oxides were good protective coatings.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
EP87302029A 1986-03-10 1987-03-10 Revêtement de protection pour films de protection solaire Expired - Lifetime EP0239280B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US837774 1986-03-10
US06/837,774 US4690871A (en) 1986-03-10 1986-03-10 Protective overcoat of titanium nitride films

Publications (3)

Publication Number Publication Date
EP0239280A2 true EP0239280A2 (fr) 1987-09-30
EP0239280A3 EP0239280A3 (en) 1989-03-22
EP0239280B1 EP0239280B1 (fr) 1993-01-27

Family

ID=25275380

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87302029A Expired - Lifetime EP0239280B1 (fr) 1986-03-10 1987-03-10 Revêtement de protection pour films de protection solaire

Country Status (10)

Country Link
US (1) US4690871A (fr)
EP (1) EP0239280B1 (fr)
JP (1) JP2857147B2 (fr)
AU (1) AU597338B2 (fr)
BR (1) BR8701087A (fr)
CA (1) CA1327295C (fr)
DE (1) DE3783790T2 (fr)
DK (1) DK168664B1 (fr)
ES (1) ES2004545A6 (fr)
MX (1) MX164217B (fr)

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0338849A2 (fr) * 1988-04-22 1989-10-25 Gec-Marconi Limited Dispositifs optiques
DE4006029A1 (de) * 1989-02-27 1990-08-30 Central Glass Co Ltd Waermereflektierendes glas mit mehrlagen-beschichtung
DE3941797A1 (de) * 1989-12-19 1991-06-20 Leybold Ag Belag, bestehend aus einem optisch wirkenden schichtsystem, fuer substrate, wobei das schichtsystem insbesondere eine hohe antireflexwirkung aufweist, und verfahren zur herstellung des belags
DE3942990A1 (de) * 1989-12-19 1991-06-20 Leybold Ag Belag, bestehend aus einem optisch wirkenden schichtsystem, fuer substrate, wobei das schichtsystem insbesondere eine hohe antireflexwirkung aufweist, und verfahren zur herstellung des belags
US5135808A (en) * 1990-09-27 1992-08-04 Diamonex, Incorporated Abrasion wear resistant coated substrate product
EP0511901A1 (fr) * 1991-04-30 1992-11-04 Saint-Gobain Vitrage Substrat en verre revêtu de multicouches minces pour la protection solaire
FR2676048A1 (fr) * 1991-04-30 1992-11-06 Saint Gobain Vitrage Int Substrat en verre revetu de multicouches minces metalliques pour la protection solaire.
FR2676047A1 (fr) * 1991-04-30 1992-11-06 Saint Gobain Vitrage Int Substrat en verre revetu de multicouches minces metalliques pour la protection solaire.
US5190807A (en) * 1990-10-18 1993-03-02 Diamonex, Incorporated Abrasion wear resistant polymeric substrate product
EP0536607A2 (fr) * 1991-09-30 1993-04-14 Ppg Industries, Inc. Revêtements d'aspects métalliques propres au traitement thermique
WO1993007099A1 (fr) * 1991-10-11 1993-04-15 Caradon Everest Limited Verre resistant au feu
EP0632294A1 (fr) * 1993-04-28 1995-01-04 The Boc Group, Inc. Miroirs
US5514454A (en) * 1993-11-02 1996-05-07 Saint-Gobain Vitrage Transparent substrate provided with a metal nitride layer
US5527596A (en) * 1990-09-27 1996-06-18 Diamonex, Incorporated Abrasion wear resistant coated substrate product
US5552180A (en) * 1991-11-29 1996-09-03 Ppg Industries, Inc. Multilayer heat processable vacuum coatings with metallic properties
US5637353A (en) * 1990-09-27 1997-06-10 Monsanto Company Abrasion wear resistant coated substrate product
US5705278A (en) * 1991-09-30 1998-01-06 Ppg Industries, Inc. Heat processable metallic vacuum coatings
US5709938A (en) * 1991-11-29 1998-01-20 Ppg Industries, Inc. Cathode targets of silicon and transition metal
US5965278A (en) * 1993-04-02 1999-10-12 Ppg Industries Ohio, Inc. Method of making cathode targets comprising silicon
US6793781B2 (en) 1991-11-29 2004-09-21 Ppg Industries Ohio, Inc. Cathode targets of silicon and transition metal
WO2023209052A1 (fr) 2022-04-28 2023-11-02 Saint-Gobain Glass France Substrat transparent muni d'un empilement fonctionnel de couches minces

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JPS63265846A (ja) * 1987-04-22 1988-11-02 Nippon Sheet Glass Co Ltd 曲げ熱線反射ガラス及びその製造方法
JPH0764598B2 (ja) * 1987-12-01 1995-07-12 旭硝子株式会社 赤外線遮断ガラス
JPH0635331B2 (ja) * 1988-02-15 1994-05-11 日本板硝子株式会社 金色反射色を有する透明板
JP2518116B2 (ja) * 1988-03-03 1996-07-24 旭硝子株式会社 耐久性の優れた光学体の製造方法
US5057375A (en) * 1988-04-15 1991-10-15 Gordon Roy G Titanium silicide-coated glass windows
US5112693A (en) * 1988-10-03 1992-05-12 Ppg Industries, Inc. Low reflectance, highly saturated colored coating for monolithic glazing
FR2640257B1 (fr) * 1988-12-08 1992-08-28 Saint Gobain Vitrage Vitrage de protection solaire monolithique
JPH0764599B2 (ja) * 1988-12-20 1995-07-12 旭硝子株式会社 耐久性の優れた熱線反射性を有する光学体
JP2637804B2 (ja) * 1988-12-20 1997-08-06 日本碍子株式会社 メッキ付き基材
US5217753A (en) * 1989-02-21 1993-06-08 Libbey-Owens-Ford Co. Coated glass articles
EP0402075B1 (fr) * 1989-06-06 1994-04-20 Nippon Sheet Glass Co., Ltd. Verre absorbant les rayons thermiques
DE4117257B4 (de) * 1989-12-27 2006-03-30 Unaxis Deutschland Holding Gmbh Optisch wirkendes Schichtsystem mit hoher Antireflexwirkung für transparente Substrate
US5215832A (en) * 1990-04-25 1993-06-01 Cardinal Ic Company Lead-free mirrors and environmentally safe manufacture thereof
WO1991016197A1 (fr) * 1990-04-25 1991-10-31 Cardinal Ig Company Miroirs sans plomb et leur fabrication sans danger pour l'environnement
US5407733A (en) * 1990-08-10 1995-04-18 Viratec Thin Films, Inc. Electrically-conductive, light-attenuating antireflection coating
US5091244A (en) * 1990-08-10 1992-02-25 Viratec Thin Films, Inc. Electrically-conductive, light-attenuating antireflection coating
DE4033881A1 (de) * 1990-10-25 1992-04-30 Leybold Ag Verfahren zur herstellung von scheiben mit einer vorgegebenen transmission
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JP3139031B2 (ja) * 1991-02-21 2001-02-26 日本板硝子株式会社 熱線遮蔽ガラス
EP0507236A3 (fr) * 1991-04-04 1992-10-21 Asahi Glass Company Ltd. Produit transparent non-iridescent
JPH0818849B2 (ja) * 1991-08-29 1996-02-28 日本板硝子株式会社 熱線遮蔽ガラス
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US5229194A (en) * 1991-12-09 1993-07-20 Guardian Industries Corp. Heat treatable sputter-coated glass systems
GB9127268D0 (en) * 1991-12-23 1992-02-19 Glaverbel Coated glass
EP0548972B1 (fr) * 1991-12-26 1997-04-23 Asahi Glass Company Ltd. Un substrat transparent revêtu d'un film
GB9414957D0 (en) * 1994-07-25 1994-09-14 Glaverbel A pyrolytically coated glazing panel
JP4058822B2 (ja) * 1997-09-30 2008-03-12 住友金属鉱山株式会社 選択透過膜用塗布液、選択透過膜および選択透過多層膜
JP2000171601A (ja) * 1998-12-08 2000-06-23 Sony Corp 反射防止膜および表示装置
US6650478B1 (en) * 1999-08-20 2003-11-18 Cpfilms Inc. Optical filter for a window
DE19948839A1 (de) 1999-10-11 2001-04-12 Bps Alzenau Gmbh Leitende transparente Schichten und Verfahren zu ihrer Herstellung
US6881487B2 (en) * 2002-11-15 2005-04-19 Guardian Industries Corp. Heat treatable coated articles with zirconium or zirconium nitride layer and methods of making same
WO2005073428A1 (fr) * 2004-01-23 2005-08-11 Arkema Inc. Procede de depot d'empilements de films sur un substrat
US8855270B2 (en) 2012-03-06 2014-10-07 General Electric Company Antiwetting coating for liquid metal bearing and method of making same
US8986921B2 (en) 2013-01-15 2015-03-24 International Business Machines Corporation Lithographic material stack including a metal-compound hard mask
US8853095B1 (en) 2013-05-30 2014-10-07 International Business Machines Corporation Hybrid hard mask for damascene and dual damascene
US11097974B2 (en) 2014-07-31 2021-08-24 Corning Incorporated Thermally strengthened consumer electronic glass and related systems and methods
JP6459373B2 (ja) * 2014-10-14 2019-01-30 Ａｇｃ株式会社 積層膜付き透明基板およびその製造方法
JP6459374B2 (ja) * 2014-10-14 2019-01-30 Ａｇｃ株式会社 窓ガラスおよび積層膜付き透明基板
WO2017123573A2 (fr) 2016-01-12 2017-07-20 Corning Incorporated Articles à base de verre fin renforcé chimiquement et thermiquement
US11795102B2 (en) 2016-01-26 2023-10-24 Corning Incorporated Non-contact coated glass and related coating system and method
US10294147B2 (en) 2017-01-05 2019-05-21 Guardian Glass, LLC Heat treatable coated article having titanium nitride based IR reflecting layer(s)
US10214956B2 (en) * 2017-01-05 2019-02-26 Guardian Glass, LLC Heat treatable coated article having titanium nitride and nickel chrome based IR reflecting layers
JP6631686B2 (ja) * 2018-12-20 2020-01-15 Ａｇｃ株式会社 積層膜付き透明基板および窓ガラス
CN113727954A (zh) 2019-04-23 2021-11-30 康宁股份有限公司 具有确定的应力分布曲线的玻璃层叠物及其制作方法
WO2021025981A1 (fr) 2019-08-06 2021-02-11 Corning Incorporated Stratifié de verre ayant des pointes de contrainte enfouies pour arrêter les fissures et procédés de fabrication associé

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Cited By (34)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0338849A3 (fr) * 1988-04-22 1990-02-28 Gec-Marconi Limited Dispositifs optiques
EP0338849A2 (fr) * 1988-04-22 1989-10-25 Gec-Marconi Limited Dispositifs optiques
US5085926A (en) * 1989-02-27 1992-02-04 Central Glass Company, Limited Neat reflecting glass with multilayer coating
DE4006029A1 (de) * 1989-02-27 1990-08-30 Central Glass Co Ltd Waermereflektierendes glas mit mehrlagen-beschichtung
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Also Published As

Publication number Publication date
CA1327295C (fr) 1994-03-01
JPS62216943A (ja) 1987-09-24
EP0239280A3 (en) 1989-03-22
AU597338B2 (en) 1990-05-31
JP2857147B2 (ja) 1999-02-10
DK120587D0 (da) 1987-03-09
DK120587A (da) 1987-09-11
ES2004545A6 (es) 1989-01-16
BR8701087A (pt) 1987-12-29
EP0239280B1 (fr) 1993-01-27
US4690871A (en) 1987-09-01
DE3783790D1 (de) 1993-03-11
DK168664B1 (da) 1994-05-16
DE3783790T2 (de) 1993-08-19
MX164217B (es) 1992-07-27
AU6954987A (en) 1987-09-17

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